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Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate

A technology for synthesizing dimethyl oxalate and dimethyl carbonate, which is applied in the preparation of carbonate/haloformate, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as failure to handle well

Active Publication Date: 2011-02-23
SHANGHAI HUAYI ENERGY CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, none of the existing technologies can handle this problem well.

Method used

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  • Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate
  • Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate
  • Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] The present embodiment is the scale of annual output of 5000 tons of dimethyl oxalate.

[0084] CO is 98.5% pure, the rest as N 2 .

[0085] o 2 The purity is also 98.5%, the rest is N 2 .

[0086] The purity of methanol is 99.9%, and the rest is water.

[0087] Supplementing NO is supplemented by the method of generating methyl nitrite from sodium nitrite, sulfuric acid and methanol.

[0088] In this example, the composition of the purge gas is: NO = 15%, CO = 10%, nitrite = 2%, methanol = 8%, N 2 = 65%. From raw gas CO and O 2 N brought into the system 2 The exhausted NO loss is 0.052 kmol / h, the CO loss is 0.03 kmol / h, and the methanol is 0.03 kmol / h.

[0089] In addition, in the nitrosation reactor, the selectivity of producing nitric acid is 2%, therefore, the amount of nitric acid produced per hour is 0.17 kmol / h, and the equivalent loss of NO is 0.17 kmol / h. It can be seen that the total NO loss is 0.22kmol / h, which is supplemented by the reaction of so...

Embodiment 2

[0103] The present embodiment is the scale of annual production of 10,000 tons of dimethyl oxalate.

[0104] CO is 98.5% pure and the remainder is N2.

[0105] The O2 purity is also 98.5%, and the rest is N2.

[0106] The purity of methanol is 99.9%, and the rest is water.

[0107] The method of supplementing NO is supplemented by ammonia oxidation.

[0108] In this example, the composition of the purge gas was: NO = 10%, CO = 10%, nitrite = 1%, methanol = 5%, and N2 was 74%. The N2 brought into the system by the raw material gas CO and O2 is 0.4kmol / h, and it is discharged through the purge gas. The NO loss is 0.073kmol / h, the CO loss is 0.073kmol / h, and the methanol is 0.036kmol / h.

[0109] In addition, in the nitrosation reactor, the selectivity of producing nitric acid is 1.2%, therefore, the amount of nitric acid produced per hour is 0.2 kmol / h, and the equivalent loss of NO is 0.2 kmol / h. It can be seen that the total NO loss is 0.273kmol / h, supplemented by the ammon...

Embodiment 3

[0123] The present embodiment is the scale of annual production of 1000 tons of dimethyl oxalate.

[0124] CO is 98.5% pure and the remainder is N2.

[0125] The O2 purity is also 98.5%, and the rest is N2.

[0126] The purity of methanol is 99.9%, and the rest is water.

[0127] The method of supplementing NO is supplementing with purchased NO cylinder gas.

[0128] In this example, the composition of the purge gas is: NO = 20%, CO = 10%, nitrite = 3%, methanol = 10%, N2 is 57%. The N2 brought into the system by the raw material gas CO and O2 is 0.04kmol / h, and it is discharged through the purge gas. The NO loss is 0.016kmol / h, the CO loss is 0.007kmol / h, and the methanol is 0.007kmol / h.

[0129] In addition, in the nitrosation reactor, the selectivity of producing nitric acid is 2.0%, therefore, the amount of nitric acid produced per hour is 0.02 kmol / h, and the equivalent loss of NO is 0.02 kmol / h. It can be seen that the total NO loss is 0.036kmol / h, equivalent to 0.81...

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Abstract

The invention discloses a method for synthesizing dimethyl oxalate and by-producing dimethyl carbonate, which adopts industrial grade CO and O2 with a purity of more than 98 percent and industrial grade methanol with a purity higher than 99.5 percent as raw materials and NO as auxiliary material, so as to prepare dimethyl oxalate and by-produce dimethyl carbonate through nitrosation, oxidative carbonylation, and extraction and rectification circulation. The invention comprises four circulation loops: an NO / CH3ONO circulation loop consisting of an oxidative carbonylation reactor and a nitrosation reactor, a methanol circulation loop 1 consisting of a nitrosation reactor and a water separation tower, a water / steam circulation loop consisting of an oxidative carbonylation reactor and a nitrosation reactor, and a methanol circulation loop consisting of a methanol cleaning tower and a methanol circulation tower. The invention provides a method used for synthesizing dimethyl oxalate and by-producing dimethyl carbonate from the CO with industrialized development value.

Description

technical field [0001] The present invention relates to a kind of method of synthesizing dimethyl oxalate, more specifically relate to a kind of method of large-scale industrialization synthesizing dimethyl oxalate and simultaneously by-product dimethyl carbonate. Background technique [0002] Dimethyl oxalate has important uses in the chemical industry. The traditional synthesis method of dimethyl oxalate is to utilize the esterification reaction of oxalic acid and methanol, which has the problems of large waste water discharge, serious environmental pollution and prominent waste of raw materials. In 1980, Japanese UBE Corporation (EP0046598, 1981; EP0086370, 1983) and U.S. Union Carbide Corporation (EP0057630, 1982) successively disclosed using CO as a raw material, by means of methyl nitrite or ethyl nitrite, and using Pd / a-Al 2 o 3 As a catalyst, the method of coupling CO oxidation to generate dimethyl oxalate or diethyl oxalate, while the Fujian Institute of Matter ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/36C07C69/96C07C67/36C07C68/00
Inventor 肖文德江志东吴良泉鲁文质黄飚单文波肖招金
Owner SHANGHAI HUAYI ENERGY CHEM
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